Cross-calibration between beta and gamma sources using quartz OSL: Consequences of the use of the SAR protocol in optical dating

The radiation dose delivered by the ⁹⁰Sr beta source of a TL-OSL reader and the one delivered by a ¹³⁷Cs gamma source were compared using OSL dating techniques and tools. Three sets of quartz of different origins (rock, sediment and loess) were studied and measured by the SAR protocol (Single aliquot regenerative dose protocol) after irradiations carried out either by the ⁹⁰Sr source or by a ¹³⁷Cs source. Measurements show that the values obtained by the SAR protocol must be corrected in order to provide an acceptable cross-calibration of the beta and gamma source. Once applied, measurement sets become self-consistent and compatible with expected values. The consequences of the above mentioned observations on the methodology of OSL dating are discussed and suggest that a mixed protocol be used including both the SAR protocol and an added dose techniques close to the SARA protocol (Single aliquot regenerative and added dose protocol).     

Bleaching of the post-IR IRSL signal from individual grains of K-feldspar: Implications for single-grain dating

Post-IR IRSL (pIRIR) signals from K-feldspar grains measured at elevated temperatures are increasingly being used for dating sediments. Unfortunately the pIRIR signal from K-feldspars bleaches more slowly than other signals (e.g. OSL from quartz) upon exposure to daylight, leading to concerns about residual signals remaining at deposition. However, earlier studies have not assessed whether the pIRIR signal bleaches at the same rate in all feldspar grains. In this study laboratory bleaching experiments have been conducted and for the first time the results show that the rate at which the pIRIR signal from individual K-feldspar grains bleach varies. To determine whether grain-to-grain variability in bleaching rate has a dominant control on equivalent dose (D_e) distributions determined using single grains, analysis was undertaken on three samples with independent age control from different depositional environments (two aeolian and one glaciofluvial). The D_e value determined from each grain was compared with the rate at which the pIRIR₂₂₅ signal from the grain bleaches. The bleaching rate of each grain was assessed by giving a 52 Gy dose and measuring the residual D_e after bleaching for an hour in a solar simulator. There is no clear relationship between the rate at which the pIRIR₂₂₅ signal of an individual grain bleaches and the magnitude of its D_e. It is concluded that variability in the bleaching rate of the pIRIR₂₂₅ signal from one grain to another does not appear to be a dominant control on single grain D_e distributions.     

Luminescence dating of quartz using an improved single-aliquot regenerative-dose protocol

Single aliquot protocols are now widely used as a means of measuring the equivalent dose (D_e) in quartz and feldspar optical stimulated luminescence (OSL) dating of both heated and sedimentary materials. The most recent of these is the single-aliquot regenerative-dose (SAR) protocol, first suggested by Murray and Roberts (Radiation Measurements 29, 503–515, 1998). In this approach, each natural or regenerated dose OSL measurement is corrected for changes in sensitivity using the OSL response to a subsequent test dose (10–20% of D_e). If the sensitivity correction is adequate, then the corrected OSL response should be independent of prior dose and thermal/optical treatment, i.e. there should be no change in the sensitivity-corrected dose–response curve on remeasurement. Here we examine the interpretation of the sensitivity corrected growth curve as a function of dose, and the effect of changing measurement conditions (e.g. preheat temperature, size of test dose, stimulation temperature) on the estimation of D_e. The dependence of the dose response on prior treatment is tested explicitly, and the significance of thermal transfer discussed. It is concluded that a robust SAR protocol is now available for quartz, and that it is applicable to a wide range of heated and unheated materials.     

Optical dating of single sand-sized grains of quartz: sources of variability

Optically stimulated luminescence (OSL) measurements have been made of over 3000 sand-sized grains of quartz. Analysis at this scale highlights the variability in the luminescence sensitivity and the dose saturation characteristics of individual quartz grains. Using a new instrument capable of measuring single grains it is feasible to routinely measure the equivalent dose from many hundreds of grains from each sample. Analysis of such datasets requires assessment of the uncertainties on each equivalent dose since these may vary significantly. This paper assesses the significance of signal intensity, dose saturation characteristics and instrument uncertainty in equivalent dose calculation.     

Assessment of diagnostic tests for evaluating the reliability of SAR De values from polymineral and quartz fine grains

In this study, we applied optically stimulated luminescence (OSL) dating to two fine grain sediment samples collected at Jeongokri, Korea. A single aliquot regenerative dose (SAR) procedure was applied to both polymineral grains and to chemically isolated (H₂SiF₆) quartz grains of 4–11 μm diameter. For polymineral fine grains, the OSL IR depletion ratio and the equivalent dose (D_e) plateau test appear to be equally sensitive indicators of appropriate IR stimulation time for use in the ‘double SAR’ protocol. Additionally, the OSL IR depletion ratio test gives an indication of the relative mineral composition of the samples, hence providing an assessment of the likelihood of obtaining a quartz-dominated [post-IR] OSL signal. Use of higher preheat temperatures would assist in thermally eroding the non-quartz component of the [post-IR] OSL signal from polyminerals. For the quartz fine grains, data from both natural D_e determinations and laboratory dose recovery tests are required to identify the appropriate preheat temperatures for dating, due to problems of thermal transfer. This phenomenon is particularly exaggerated for these samples due to the large D_e values (≥350 Gy) and hence low slope of the dose–response curve. The double SAR method cannot be applied ubiquitously, even after careful and rigorous study of one sample from a section. Quartz OSL dating using a range of preheat temperatures is suggested to be the most suitable method for OSL dating of fine grain sediments.     

The problem of dating quartz 2: Synchrotron generated X-ray excited optical luminescence (XEOL) from quartz

The luminescence emission of quartz is used in optically stimulated luminescence dating (OSL), however the precise origins of the emission are unclear. A suite of quartz samples were analysed using X-ray excited optical luminescence (XEOL). Radiation dose effects were observed whereby the UV emissions (3.8 and 3.4 eV) were depleted to the benefit of the red emission (1.9–2.0 eV). Samples were excited at ∼7 keV. Understanding why some quartz emit light more brightly than others will increase the efficiency and precision of OSL analyses.     

Investigations of the post-IR IRSL protocol applied to single K-feldspar grains from fluvial sediment samples

The post-IR IRSL protocol with single K-feldspar grains was applied to three samples taken from a fluvial sedimentary sequence at the archaeological site of the Dali Man, Shaanxi Province, China. K-feldspar coarse grains were extracted for measurement. Approximately 30–40% of the grains were sufficiently bright to measure, and after application of rejection criteria based on signal strength, recuperation, recycling ratio and saturation dose, ～10–15% of the grains were used for D_e calculation. The relationship of signal decay rate and form of D_e(t) with the recovery dose were investigated. The dose recovery ratios of the samples after initial bleaching with the four different light sources were within uncertainties of unity. No anomalous fading was observed. The over-dispersion of the recovered dose and D_e values were similar, suggesting neither incomplete resetting of the post-IR IRSL signals nor spatially heterogeneous dose rates significantly affected the natural dose estimates. The values of D_e obtained with the single K-feldspar grain post-IR IRSL protocol were in the range ～400–490 Gy. Combining all of the measured single-grain signals for each of the individual samples (into a ‘synthetic single aliquot’) increased the D_e estimates to the range ～700–900 Gy, suggesting that the grains screened-out by the rejection criteria may have the potential to cause palaeodose over-estimation, although this finding requires a more extensive investigation. Thermally transferred signals were found in the single K-feldspar grains post-IR IRSL protocol, and the proportion of thermally transferred signal to test-dose OSL signal (stimulation at 290 °C) from the natural dose was higher than from regenerative doses, and the proportion was grain- and dose-dependent. As such, TT-post-IR IRSL signals at 290 °C have the potential to cause dose underestimation, although this may be reduced by using larger test-dose irradiations. Our study demonstrates considerable potential in the post-IR IRSL method in providing chronological control in studies relevant to human evolution in the later-Pleistocene.     

Palaeodose underestimates caused by extended-duration preheats in the optical dating of quartz

An optical dating study of some quartzose sediments from northern and southern Australia, north Africa and north-western Europe has revealed that palaeodose (P) underestimates of 10–40% are obtained when an extended-duration preheat of 160°C for 16 h is used. For these samples in the 0–60 ka age range, a preheat of 220°C for 5 min produces the correct P, as inferred from the concordance with thermoluminescence (TL) palaeodose determinations on the same sedimentary sample or on burnt flint. Independent support for use of the 220°C preheat is given by the agreement between optical ages younger than 30 ka and ¹⁴C age determinations on associated charcoal. The deleterious effect of the 160°C preheat is illustrated by growth curves of optically stimulated luminescence (OSL) vs added dose. These curves show that the 160°C preheat induces a dose-dependent increase in sample sensitivity, which may be related to activation of the pre-dose mechanism. The 160°C preheat also causes low-dose supralinearity, although the supralinearity correction is insufficient to reduce significantly the degree of P underestimation. A normalization method based on preheat-induced sensitivity changes of the 110°C TL peak, albeit limited by saturation effects, warrants further investigation.     

Circumventing possible inaccuracies of the single aliquot regeneration method for the optical dating of quartz

A simple method of assessing the reliability of the single aliquot regeneration method is presented, based on the repeated measurement of identical regeneration doses. It is shown that for the majority of the samples measured the requirement of a constant repeat point in each cycle is not met. The ability to maintain a constant repeat point is shown to be dependent upon preheating conditions, the requirements for which were found to vary at both inter-sample and inter-aliquot levels. The expected effect on estimated values of D_e is calculated and shown to be significant. Three possible means of circumventing these inaccuracies are presented: (i) adjustment of the measurement procedure (specifically the preheat conditions); (ii) modelling and correcting for the effect, and (iii) stabilising the response prior to construction of the regenerated growth curve. It is suggested that much of the variation in D_e observed between individual aliquots and between individual grains from well-bleached sediments may possibly be attributed to differences in preheating requirements, and that such differences may also account for some of the spread in D_e for partially bleached sediments.     

Determination of burial dose in incompletely bleached fluvial samples using single grains of quartz

We determine the burial dose in three known-age incompletely bleached fluvial samples using single grains of quartz. Estimation of burial dose in incompletely bleached samples requires that the characteristics of the well-bleached part of the distribution are known in order to distinguish between well-bleached and poorly bleached grains. It is especially important to investigate if the uncertainties assigned to individual estimates of dose adequately describe the observed variability in well-bleached dose distributions. We investigate this by quantifying the over-dispersion in laboratory-bleached and gamma-irradiated samples. We show that there is a linear relationship between the over-dispersion and the mean dose. Knowing this uncertainty relationship enables us to estimate the burial dose by comparing the predicted uncertainty on the running mean with that calculated from actual dispersion.     

Dosimetric properties of natural quartz grains extracted from fired materials

The paper describes an examination of the dosimetric properties of natural quartz grains extracted from ancient fired materials. Eleven samples of different origin were tested for their TL and GLSL (green light stimulated luminescence) sensitivities within the mGy dose range. Very promising results were obtained showing the possibility of measuring the doses of around 10 mGy with 1% precision using GLSL or TL and using the single aliqout technique for natural quartz as a dosimeter. The lowest detectable dose was estimated to be lower than 500 μGy. The results obtained indicate that natural quartz grains from selected materials could be used for the dosimetry of environmental gamma radiation for the purposes of paleodosimetric dating methods as well as for accident dosimetry.     

On the dependence of equivalent dose on temperature of OSL measurements for sediment quartz grains and its implication in dating practice

The dependence of the equivalent dose (D_e) on the temperature used at stimulation when the standard OSL dating protocol (SAR) is applied has been investigated for sediment quartz samples. A considerable change in this value appears in the temperature region from 80 to 140 °C that is known for high complexity in OSL processes in quartz. Our observations suggest that the variation in the obtained results at least partly is caused by the laboratory procedure used when the natural OSL signal is measured. Directions for further investigations concerning this undesirable effect are indicated.     

Reliability of single aliquot regenerative protocol (SAR) for dose estimation in quartz at different burial temperatures: A simulation study

The single aliquot regenerative protocol (SAR) is a well-established technique for estimating naturally acquired radiation doses in quartz. This simulation work examines the reliability of SAR protocol for samples which experienced different ambient temperatures in nature in the range of −10 to 40 °C. The contribution of various experimental variables used in SAR protocols to the accuracy and precision of the method is simulated for different ambient temperatures. Specifically the effects of paleo-dose, test dose, pre-heating temperature and cut-heat temperature on the accuracy of equivalent dose (ED) estimation are simulated by using random combinations of the concentrations of traps and centers using a previously published comprehensive quartz model. The findings suggest that the ambient temperature has a significant bearing on the reliability of natural dose estimation using SAR protocol, especially for ambient temperatures above 0 °C. The main source of these inaccuracies seems to be thermal sensitization of the quartz samples caused by the well-known thermal transfer of holes between luminescence centers in quartz. The simulations suggest that most of this inaccuracy in the dose estimation can be removed by delivering the laboratory doses in pulses (pulsed irradiation procedures).     

Study of the 110°C TL peak sensitivity in optical dating of quartz

As the 110°C TL emission in quartz uses the same luminescence centers as the OSL emission, the 110°C TL signal from a test dose may be used to monitor the OSL sensitivity change. It is thus important to study the relationship between the 110°C TL peak and the OSL sensitivity in studies related to optical dating from quartz. We have conducted a series of experiments using sedimentary quartz, where the annealing temperatures were varied between 260 and 1000°C before the measurement of OSL and 110°C TL sensitivities. Another series of experiments on two sedimentary quartz samples investigated the 110°C TL peak and OSL dose-dependent sensitivity change after different annealing temperatures. In these experiments, the 110°C TL and OSL signals from the test dose are shown to have similar sensitization characteristics: the 110°C TL sensitivity change is proportional to the OSL sensitivity change if the annealing temperature is lower than 500°C. It is concluded that the 110°C TL signal can be used to correct the OSL sensitivity change in the single-aliquot additive-dose protocol.     

Extending the age range of optical dating using single ‘supergrains’ of quartz

Luminescence dating methods have been used to obtain reliable age estimates for quartz sediments deposited within the last 500 ka, but it has proven difficult to extend the age range much beyond this limit. Here we report the results of a study of individual quartz grains from Australian sedimentary deposits that range in age from 250 to 950 ka. A small number of the grains examined are strongly luminescent and saturate at unusually high doses. These ‘supergrains’ may permit reliable age determination to 1 Ma, and possibly beyond. Some other grains are in, or close to, dose-saturation, so that only minimum age estimates may be obtained. Most of the grains examined are very weakly luminescent and have palaeodoses much less than expected, while the palaeodoses of some grains cannot be estimated because of anomalous dose–response characteristics. We offer some possible explanations for the behaviour of aberrant grains.     

Distinguishing dose populations in sediment mixtures: a test of single-grain optical dating procedures using mixtures of laboratory-dosed quartz

Many natural deposits contain grains that have different burial histories, but reliable procedures to extract the component doses from mixed-dose samples have not been developed in optical dating. Here we present results for synthetic two- and three-component mixtures of data derived from laboratory-dosed sedimentary quartz using a single-aliquot regenerative-dose protocol and statistical models for finite mixtures. Composite sets of data were created from the doses measured for individual grains that had been bleached by sunlight and then given a beta dose of 5, 10 or 20 Gy. We found that the correct number of dose components, corresponding doses, and relative proportions of each component may be estimated if the within-component dispersion is small or is known. We also found, however, that recuperation of the OSL signal in sun-bleached quartz may produce artificially high dose estimates for some grains, an effect that should be taken into account when modelling natural mixtures.     

A study of thermoluminescence emission spectra and optical stimulation spectra of quartz from different provenances

The present study examines (1) variability in the thermoluminescence (TL) emission spectrum and optical stimulation (OSL) spectrum of quartz from different provenances and, (2) possible correlations between spectral features and the nature of the complex growth curves (ranging from saturating exponential to those described by a cubic polynomial function), so as to determine the validity of the currently used experimental protocols. The results suggest that commonly used UV emission for dating constitutes only a minor component of the total quartz emission and in view of this a dose-dependent contribution from blue/blue–green emission peak to the UV detection is likely. The OSL stimulation spectrum shows a definite change in stimulation response between 500–520 nm, hence implying that stimulation in this window may contribute as an additional source of scatter in multi-grain samples.     

Zeroing of the OSL signal in quartz from young glaciofluvial sediments

The natural luminescence of quartz samples from recent (<200 yr old) glaciofluvial sediments collected from a range of distances from the snout of the Gangotri glacier in the Garhwal Himalaya, India, was measured. Six measured D_E (equivalent dose) values ranged from 35 to 175 Gy, strongly suggesting that these samples had been exposed to daylight only poorly before deposition. However, regenerated growth curves constructed after exposure to several hours of natural daylight gave apparent D_E values ranging from 10 to 30 Gy. Detailed measurements of one sample confirm that these observations are due to a huge recuperation effect. The “shine plateaux” observed in the majority of these D_E determinations showed little increase of D_E with increasing exposure time. The mechanisms of this unexpected behaviour, and the implications for the detection of partial bleaching, are discussed.     

A novel multipriority reservation protocol for plastic optical fiber access network

In this paper, a novel multipriority reservation protocol for plastic optical fiber access network based on optical code division multiplexing access (OCDMA) technology is proposed. Conventional OCDMA system only allows finite units to transmit and access simultaneously according to the number of channels. The protocol is proposed to resolve this problem. By using the reservation scheme and a distributed arbitration algorithm, channel collision and destination conflict can be avoided. The protocol can efficiently support the transmission of multimedia messages that require the different time-delays. At the same time, each optical network unit is equipped with a fixed optical encoder/decoder that is always tuned to channel for control and the tunable optical encoder/decoder that is tuned to any of channel for data. The network throughput and average delay have been investigated by numerical analysis and simulation experiments. It is shown that the multipriority reservation protocol in this POF access net